Treatment of textile and other materials



Patented Nov. 3, 12

Richard R. Sitzler, cum

d, Md, assignor to lanese Corporation America. a corporation of Delaware No Drawing. Application October 19, 1940, Serial N0. 361,897

This invention relates to the preparation of artificial materials of improved properties, and relates more particularly to the preparation of colored filaments, yarns and other textile materials containing titanium dioxide which are fast to light. I

Artificial filaments, yarns and other textile ma= terials of low luster have been prepared with the aid of titanium dioxide by incorporating the titanium dioxide in the spinning solution from which artificial filaments or yarns are spun or by incorporating the titanium dioxide or hydrated titanium dioxide in the already spun filaments or yarns, for example, by interaction of suitable reagents on the filaments or yarns by treating the filaments or yarns with an aqueous dispersion of titanium dioxide. It has been found, however, that when artificial filaments, yarns or fabrics containing titanium dioxide are colored, the colors are generally not as fast to light as those yielded by the same dyestuffs upon similar materials free from titanium dioxide. This lack of light fastness is particularly noticeable in the case of drapery fabrics that are exposed to sunlight. Not only do the colors fade but the materials also frequently lose strength.

It is, accordingly, an important object of this invention to prepare artificial filaments, yarns and-other textile material containing titanium dioxide which do not deteriorate when exposed to simlight.

Another object of this invention is to prepare colored artificial filaments, yarns and other textile materials containing titanium dioxide which do not fade or lose strength after long exposure to light.

Other objects of this invention will appear from the following detailed description.

As stated, colored artificial filaments, yarns or fabrics containing titanium dioxide are normally neither as light-last or as strong as'colored materials which are free from titanium dioxide. Many expedients have been tried to obviate or to minimize the undesirable effects of titanium dioxide. For example, in U. S. Patent No. 2,206,278 to Henry Dreyfus there is described a process for improving the light-fastness and strength of colored materials containing titanium dioxide wherein the titanium dioxide is associated or treated with a compound of manganese, iron, cobalt, nickel or copper. While fairly good results may be obtained by the process of this patent, I have found that superior results may be obtained by adding to the titanium dioxide small amounts of compounds of aluminum and antimony. I

In accordance with my invention, I prepare artificial filaments containing titanium dioxide of superior light-fastness and strength by associating small amounts of compounds of aluminum and antimony, preferably the oxides of these metals as they are white in color, with the titanium dioxide and then adding the same in finely divided form to the spinning solution from which the filaments are spun.

The filaments made in accordance with this invention may be of fine size and adapted to be associated together by twisting to form yarn, or the filaments may be of large cross-section such as bristles, artificial horse-hair and straw. The filaments may be made from reconstituted or regenerated cellulose by the viscose, cuprammonium, Chardonnet or other process, but this invention is of particular importance in connection with filaments made of organic derivatives of cellulose, such as organic esters of cellulose and cellulose ethers. Examples of organic esters of cellulose are cellulose acetate, cellulose propionate and cellulose butyrate, as well as mixed esters such as cellulose aceto-propionate and cellulose aceto-butyrate, while examples of cellulose ethers are ethyl cellulose and benzyl cellulose. The filaments made of organic derivative of cellulose may be prepared by dissolving the organic derivative of cellulose in a volatile solvent, such as acetone, and extruding such solutions through orifices of suitable size into an evaporative atmosphere as in dry spinning. or into a precipitating bath as in wet spinning.

The pigment comprising the titanium dioxide and the oxides of antimony and aluminum is preferably added to the spinning solution containing the cellulose compound in the form of a concentrated suspension in a liquid. The amount ofpigment added to the spinning solution will vary with the degree of subdued luster and depth of color desired and will generally be from 0.1 to 10%, based on the weight of the cellulose compound present in the finished yarn. I have found that highly satisfactory results may be obtained in the case of cellulose acetate filaments or yarns by adding to the spinning solution an amount of pigment in a proportion of 1.5% on the weight of the cellulose acetate.

It is of importancethat the pigment added to the spinning solution be in very fine form, the particles preferably having a diameter of less than 0.1 to no more than 5 microns for increased covering power and to obtain the depth of color desired without the necessity of incorporating such a large amount of pigment as to deleteriously affect the strength and other properties of the yarn. In order to obtain the desired fine size of pigment particles, I prefer to mill the pigment for about twenty-four hours in a 10% solution of the cellulose compound to be formed into filaments. In this manner, there may be obtained a suspension ofzpigment particles ranging in size from less than 0.1 micron to about 5 microns,

about of which are less than 1 micron in As stated, the amount of aluminum oxide and antimony oxide added to the titanium dioxide may be of small proportion, for example, a proportion on the order of 0.5 to 1.5%, based on the weight of the titanium dioxide of each of these oxides. I prefer, however, to employ from 0.8 to 0.85% of each of the oxides.

The process of my invention enables improved results with regard to fastness to light to be obtained when materials containing titanium dioxide are colored with dyestuffs of widely varying types. For example, the improvement is particularly good in the case of water-soluble azo dyestlifls having a substantive afllnity for regenerated cellulose. Moreover, the dyestuffs may be azo dyes, soluble or insoluble in water, having a direct afiinity for cellulose acetate. Other classes of dyes, the colorations of which on textile materials containing titanium dioxide may be improved by my process, are the amino-anthraquinone dyestuil's having direct ailinity for cellulose acetate. The improvement is also good in the case of dyes made with 1.4-diamino-anthraquinone or l.4-amino-oxy.-anthraquinone and other substitution products, for example, 1.4-di- (alkylamino) -'-anthraquinones. An improvement may even be obtained in the case of those dyestufis normally regarded as having a very high degree of fastness, e. g. dyes of the indigoid series and the water-insoluble azo dyestuffs produced on the fiber, such as those produced by coupling diazotized amines with suitable coupling compounds such as p naphthol aryl amides of 2:3-

oxy-naphthoic acid or diacyl-acetyl derivatives of aromatic diamines.

The following example illustrates the invention but it is not to be regarded as limiting it in any way: a

' Example:

' soluble cellulose acetate and 3 parts by weight of acetone in such an amount that the amount of pigment is present in a proportion equal to 1 /2% on the weight of the cellulose acetate present in said spinning solution. The solution is then spun in the normal manner through orifices of suitable size to form filaments which are then associated together to form yarn.

Fabric woven and knitted from yarns made in accordance with this invention and colored with such SRA dyes as Blue G, Blue IV, Golden Yellow IX, Orange III, Golden Orange HI and Red VI when exposed to fadeometer for a substantial period of time did not show any fading nor any loss in strength.

It is to beunderstood that the foregoing detailed description is merely given by way of illustration and that many variations may be made therein without departing from the spirit of my invention.

Having described my invention, what I desire to secure by Letters Patent is:

1. Process for improving the light-fastness and strength of colored textile materials containin titanium dioxide, which comprises incorporating antimony.

2. Process for improving the light-fastness and strength of colored artificial textile materials having a basis of cellulose'acetate and containing titanium dioxide, which comprises incorporating in the materials a pigment containing titanium dioxide associated with oxides of aluminum and antimony. V

3. Process for improving the light-fastness and strength of colored textile materials containing titanium dioxide, which comprises incorporating in the materials a pigment containing titanium dioxide associated with oxides of aluminum and antimony, each of the oxides in a proportion of from 0.5 to 1.5% based on the weight of the titanium dioxide.

4. Process'for improving the light-fastness and strength of colored artificial textile materials having a basis of cellulose acetate and containing titanium dioxide, which comprises incorporatin in the materials a pigment containing titanium dioxide associated with oxides "-of' aluminum and antimony, each. of the oxides in a proportion of from 0.5 to 1.5% based on the weight of the titanium dioxide.

5. Process for improving the light-fastness and strength of colored textile materials containing titanium dioxide, which comprises incorporating in the materials a pigment containing titanium dioxide associated 'with oxides of aluminum and antimony, each of the oxides in a proportion of from 0.8 to 0.85% based on the weight of the titaniumdioxide.

6. Process for improving the light-fastness and 'strength of colored artificial textile materials having a basis of cellolose acetate and containin titanium dioxide, which comprises incorporating in the materials a pigment containing titanium dioxide associated with oxides of aluminum and antimony, each of the oxides in a proportion of from 0.8 to 0.85% based on the weight of the titanium dioxide.

7. Process for improving the light-fastness and strength of colored artificial textile materials having a basis of cellulose acetate and containing titanium dioxide, which comprises incorporating in the materials a pigment containing titanium dioxide, aluminum oxide in a proportion of 0.81% and antimony oxide in a proportion of 0.84%, the proportions being based on the weight of the titanium dioxide.

8. A colored textile material of low luster, owing its low luster to the presence therein of a pigment consisting of titanium dioxide associated with aluminum oxide and antimony oxide.

9. A colored textile material having a basis of an organic derivative of cellulose and having a low luster, owing its low luster to the presence therein of a pigment consisting of titanium dioxide associated with aluminum oxide and antimony oxide, each of the oxides in a proportion of from 0.5 to 1.5% based on the weight of the titanium dioxide.

10. A colored textile material having a basis of cellulose acetate and having a low luster, owing its low luster to the presence therein of a pigment consisting of titanium dioxide associated with-aluminum oxide and antimony oxide, each of the oxides in a proportion of from 0.5 to 1.5% based on the weight of the titanium dioxide.

RICHARD R. SITZLER. 

